Hydrochloric Acid → 2-Amino-1-(3-methoxyphenyl)ethanone
반응식
[N:1]([CH2:4][C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][CH3:14])[CH:8]=1)=[O:6])=[N+]=[N-].[ClH:15]>[Pd].CO>[ClH:15].[NH2:1][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][CH3:14])[CH:8]=1)=[O:6]참가 물질
6
반응 조건
- 온도
- 25 °C
실험 절차
Palladium on carbon (10 wt %, 10.41 g, 9.78 mmol) was added to a solution of 2-azido-1-[3-(methyloxy)phenyl]ethanone (1.87 g, 9.78 mmol) and hydrochloric acid (8.14 mL, 98 mmol) in CH3OH (50 mL) under nitrogen, and the reaction mixture was stirred under hydrogen overnight at 25° C. The mixture was filtered, washing with CH2Cl2 (50 mL) and CH3OH (100 mL), and then concentrated. Water (150 mL) was added, and the mixture was lyophilized to afford an HCl salt of the title compound (2.0 g) as a brown solid. LC-MS (ES) m/z=166 [M+H]+.
후처리
- filtrationThe mixture was filtered
- washwashing with CH2Cl2 (50 mL) and CH3OH (100 mL)
- concentrationconcentrated
- additionWater (150 mL) was added
출처 및 근거
- ORD 기록
- ord-ab9fdc775cf34e7b93852829c5416a1a
- 출처 데이터셋
- uspto-grants-2014_04
- 특허 번호
- US08697685B2
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